HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethanolamine → HCID 86615470, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethanolamine | HCID 8113 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 57468843 | HCID 57468843 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86615470 | HCID 86615470 | 53% |
Reaction Steps
To a cooled (ice-water bath) and stirred mixture of diethanolamine (0.12 g, 1.14 mmol), triethylamine (0.06 ml, 0.42 mmol) and THF (2 ml) was added drop wise a solution of 3′-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyrimidin-2-yl]-biphenyl-3-sulfonyl chloride (example I.3) (0.21 g, 0.39 mmol) in THF (3 ml). The mixture was allowed to stir at room temperature for 16 h. Purification of the reaction mixture by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (diethyl ether/hexane) yielded the title compound as a white solid (0.125 g, 53%). MS (ISP) 611.6 [(M+H)+]; mp 111.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183262B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-b5afd2c9c4d64cd799af4448f2f7ecd7 |
| Source note | uspto-grants-2012_05 |